CN107353417B - Preparation method of polymer nano material - Google Patents
Preparation method of polymer nano material Download PDFInfo
- Publication number
- CN107353417B CN107353417B CN201710431326.3A CN201710431326A CN107353417B CN 107353417 B CN107353417 B CN 107353417B CN 201710431326 A CN201710431326 A CN 201710431326A CN 107353417 B CN107353417 B CN 107353417B
- Authority
- CN
- China
- Prior art keywords
- polymer
- acetanilide
- nano material
- organic solvent
- polymer nano
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/12—Powdering or granulating
- C08J3/14—Powdering or granulating by precipitation from solutions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08J2327/06—Homopolymers or copolymers of vinyl chloride
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2327/16—Homopolymers or copolymers of vinylidene fluoride
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention discloses a preparation method of a polymer nano material, which comprises the steps of adding a polymer into a first organic solvent, adding acetanilide, heating and stirring uniformly, pouring into distilled water to separate out white crystals, stirring uniformly, carrying out suction filtration and drying; grinding the dried white crystal, adding a second organic solvent, performing ultrasonic dispersion, performing suction filtration by using an organic microporous filter membrane, and drying to obtain the polymer nano material. The invention dissolves polymer and acetanilide in organic solvent, then pours distilled water to separate out white crystal. The polymer nano material is obtained by removing acetanilide in white crystals by using ethanol by utilizing the characteristic that acetanilide is slightly soluble in water (0.46g/100g, 20 ℃) and is easy to dissolve in ethanol (36.9g/100g, 20 ℃).
Description
Technical Field
The invention belongs to the field of nano material preparation, and particularly relates to a preparation method of a polymer nano material.
Background
Acetanilide is a raw material of sulfonamides and can be used as an analgesic, antipyretic and preservative. Used for manufacturing dye intermediates of paranitroacetanilide, paranitroaniline and p-phenylenediamine. Polyvinyl chloride, polyvinylidene fluoride and other polymers are not easy to break, have low melting point, generate agglomeration in the production process, have poor dispersibility and limit the application of the polymers.
Disclosure of Invention
The invention aims to provide a preparation method of a polymer nano material, which solves the problems that a polymer is not easy to break, has low melting point and generates agglomeration in the production process.
In order to achieve the purpose, the invention adopts the following technical scheme:
adding a polymer into a first organic solvent, adding acetanilide, heating and stirring uniformly, pouring into distilled water to separate out white crystals, filtering after stirring uniformly, and drying; and grinding the dried white crystals, adding a second organic solvent, performing ultrasonic dispersion (common ultrasonic cleaning), performing suction filtration and drying to obtain the polymer nano material.
Further, the polymer is one or two of polyvinyl chloride and polyvinylidene fluoride.
Further, the first organic solvent is one or more of tetrahydrofuran, N-dimethylformamide and N, N-dimethylacetamide.
Furthermore, the mass ratio of the polymer to the acetanilide is 1: 30-1: 300.
Further, the volume ratio of the first organic solvent to the distilled water is 1: 30-1: 50.
Further, white crystals precipitated in distilled water were stirred for 3 hours and then filtered under suction.
Further, the second organic solvent is one or two of ethanol and acetone.
Further, the heating and stirring temperature is 50-100 ℃.
Compared with the prior art, the invention has the following advantages:
1. the preparation method of the polymer nano material is simple, the related organic solvent can be further recycled, and the cost is low.
2. The invention has wide applicability and is suitable for other polymers dissolved in organic solvents, such as polyvinyl chloride, polyvinylidene fluoride and the like.
3. The polymer nano-particles can be prepared in large batch.
4. Solves the problems that the high molecular polymer is not easy to break, has low melting point and generates agglomeration in the production process.
The invention dissolves polymer and acetanilide in organic solvent, then pours distilled water to separate out white crystal. The polymer nano material is obtained by removing acetanilide in white crystals by using ethanol by utilizing the characteristic that acetanilide is slightly soluble in water (0.46g/100g, 20 ℃) and is easy to dissolve in ethanol (36.9g/100g, 20 ℃). At present, polymer particles are not easy to break, have low melting points and generate agglomeration phenomenon in the preparation process. The research of using acetanilide and polymer cocrystallization method to prepare polymer nano material has not been reported.
Drawings
FIG. 1 is a transmission electron micrograph of nanomaterials of example 1.
Detailed Description
The invention dissolves polymer and acetanilide in organic solvent, then pours distilled water to separate out white crystal, and prepares polymer nano material by acetanilide and polymer cocrystallization method: the polymer nano-particles are crystallized and separated out in water and are isolated by the crystals separated out in water by the acetanilide, and a mixture of the polymer nano-particles and the acetanilide crystals is prepared. The polymer nano material is obtained by removing the acetanilide in the white crystal by using ethanol by utilizing the characteristics that the acetanilide is slightly soluble in water and is easily soluble in the ethanol.
The invention relates to a preparation method of a polymer nano material, which comprises the following steps: adding the polymer into an organic solvent, adding acetanilide, heating and stirring for 0.5 hour, pouring into distilled water to separate out white crystals, stirring for 3 hours, then carrying out suction filtration, and drying at 50 ℃. And grinding the dried white crystals, adding ethanol, performing ultrasonic dispersion for 0.5 hour, and performing suction filtration and drying to obtain the polymer nano material.
The invention is further described below, the process steps are as follows:
1. the polymer was added to an organic solvent, and acetanilide was then added thereto, followed by heating and stirring for 0.5 hour to obtain a yellow transparent liquid.
2. Pouring the yellow transparent organic solution into distilled water, crystallizing the polymer and the acetanilide after the organic solvent is lost, separating out white crystals,
3. stirring for 3 hr to release residual organic solvent, suction filtering and stoving at 50 deg.c.
4. The dried white crystals were ground, added with ethanol and ultrasonically dispersed for 0.5 hour.
5. And (4) carrying out suction filtration by using an organic microporous filter membrane, and drying at 50 ℃ to obtain the product.
Example 1: adding 0.1g of polyvinylidene fluoride into 50mL of tetrahydrofuran, adding 30g of acetanilide, heating to 50 ℃, stirring for 0.5 hour, pouring into 1800mL of distilled water to separate out white crystals, stirring for 3 hours, carrying out suction filtration, and drying at 50 ℃. And grinding the dried white crystals, adding ethanol, performing ultrasonic dispersion for 0.5 hour, and performing suction filtration and drying to obtain the polymer nano material.
Example 2: adding 0.2g of polyvinylidene fluoride into 50mL of N, N-dimethylacetamide, adding 30g of acetanilide, heating to 100 ℃, stirring for 0.5 hour, pouring 1800mL of distilled water to separate out white crystals, stirring for 3 hours, performing suction filtration, and drying at 50 ℃. And grinding the dried white crystals, adding ethanol, performing ultrasonic dispersion for 0.5 hour, and performing suction filtration and drying to obtain the polymer nano material.
Example 3: adding 0.5g of polyvinylidene fluoride into 50mL of N, N-dimethylformamide, adding 30g of acetanilide, heating to 50 ℃, stirring for 0.5 hour, pouring into 1500mL of distilled water to separate out white crystals, stirring for 3 hours, carrying out suction filtration, and drying at 50 ℃. And grinding the dried white crystals, adding ethanol, performing ultrasonic dispersion for 0.5 hour, and performing suction filtration and drying to obtain the polymer nano material.
Example 4: adding 0.1g of polyvinyl chloride into 50mL of N, N-dimethylformamide, adding 30g of acetanilide, heating to 50 ℃, stirring for 0.5 hour, pouring into 1800mL of distilled water to separate out white crystals, stirring for 3 hours, carrying out suction filtration, and drying at 50 ℃. And grinding the dried white crystals, adding ethanol, performing ultrasonic dispersion for 0.5 hour, and performing suction filtration and drying to obtain the polymer nano material.
Example 5: adding 1g of polyvinyl chloride and 0.1g of polyvinylidene fluoride into 50mL of tetrahydrofuran, adding 30g of acetanilide, heating to 50 ℃, stirring for 0.5 hour, pouring 2500mL of distilled water to separate out white crystals, stirring for 3 hours, performing suction filtration, and drying at 50 ℃. And grinding the dried white crystals, adding ethanol, performing ultrasonic dispersion for 0.5 hour, and performing suction filtration and drying to obtain the polymer nano material. The process for preparing the polymer nano-particles is simple, the diameter of most of the particles is obviously less than 100nm, and the dispersibility is better.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (4)
1. The preparation method of the polymer nano material is characterized in that a polymer is added into a first organic solvent, acetanilide is added, the mixture is heated and stirred to be uniform, white crystals are separated out by pouring the mixture into distilled water, and the mixture is filtered, filtered and dried after being stirred uniformly; grinding the dried white crystals, adding a second organic solvent, performing ultrasonic dispersion, performing suction filtration and drying to obtain a polymer nano material;
the polymer is one or two of polyvinyl chloride and polyvinylidene fluoride;
the first organic solvent is one or more of tetrahydrofuran, N-dimethylformamide and N, N-dimethylacetamide;
the second organic solvent is ethanol.
2. The method for preparing the polymer nano material according to claim 1, wherein the mass ratio of the polymer to the acetanilide is 1: 30-1: 300.
3. The method for preparing a polymer nanomaterial according to claim 1, wherein a volume ratio of the first organic solvent to distilled water is 1:30 to 1: 50.
4. The method for preparing a polymer nanomaterial according to claim 1, wherein the white crystals precipitated in distilled water are stirred for 3 hours and then filtered under suction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710431326.3A CN107353417B (en) | 2017-06-08 | 2017-06-08 | Preparation method of polymer nano material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710431326.3A CN107353417B (en) | 2017-06-08 | 2017-06-08 | Preparation method of polymer nano material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107353417A CN107353417A (en) | 2017-11-17 |
| CN107353417B true CN107353417B (en) | 2020-03-13 |
Family
ID=60272670
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710431326.3A Expired - Fee Related CN107353417B (en) | 2017-06-08 | 2017-06-08 | Preparation method of polymer nano material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107353417B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007262158A (en) * | 2006-03-27 | 2007-10-11 | Osaka Prefecture | Microparticle of polyoxazole or its precursor and method for producing the microparticle |
| CN103044173A (en) * | 2012-12-06 | 2013-04-17 | 中国工程物理研究院化工材料研究所 | Method for preparing ordered porous energetic crystal material |
| CN105705017A (en) * | 2013-11-13 | 2016-06-22 | 日本曹达株式会社 | Co-crystal and method for producing same |
| CN105731444A (en) * | 2016-04-22 | 2016-07-06 | 武汉理工大学 | Preparation method of graphene easy to disperse |
-
2017
- 2017-06-08 CN CN201710431326.3A patent/CN107353417B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007262158A (en) * | 2006-03-27 | 2007-10-11 | Osaka Prefecture | Microparticle of polyoxazole or its precursor and method for producing the microparticle |
| CN103044173A (en) * | 2012-12-06 | 2013-04-17 | 中国工程物理研究院化工材料研究所 | Method for preparing ordered porous energetic crystal material |
| CN105705017A (en) * | 2013-11-13 | 2016-06-22 | 日本曹达株式会社 | Co-crystal and method for producing same |
| CN105731444A (en) * | 2016-04-22 | 2016-07-06 | 武汉理工大学 | Preparation method of graphene easy to disperse |
Non-Patent Citations (2)
| Title |
|---|
| "乙酰苯胺对聚氯乙烯微观结构和性能的影响";刘亚群等;《武汉理工大学学报》;20070630;第29卷(第6期);第5-7页 * |
| "小分子有机化合物对聚氯乙烯结晶度的影响";刘亚群;《化工进展》;20070228;第26卷(第2期);第249-252页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107353417A (en) | 2017-11-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN114014836A (en) | Method for purifying cyclic lactide | |
| CN102992309A (en) | Method for quickly preparing high-quality graphene oxide solids in large scale | |
| CN103130211A (en) | Preparation method of graphene | |
| CN107353417B (en) | Preparation method of polymer nano material | |
| CN107474147B (en) | Preparation method and application of macromolecular esterified water-soluble soybean polysaccharide | |
| KR101319681B1 (en) | Preparation of epsilon copper phthalocyanine of small primary particle size and narrow particle size distribution by kneading | |
| CN114163684B (en) | Method for directly extracting silk fibroin nanofibers from waste cocoons and recovering hydrolyzed silk proteins and extracting solution | |
| CN105399078A (en) | Method for preparing fluorescent carbon dots on basis of shaddock | |
| CN106167260B (en) | A kind of magnetic graphene preparation process and equipment | |
| CN110938210A (en) | Catalytic cracking slurry oil ash settling aid and preparation method thereof | |
| CN110787653B (en) | Composite membrane containing covalent organic framework material and preparation method thereof | |
| CN110256238B (en) | Refining method of long-chain mixed dibasic acid | |
| JP6768970B2 (en) | How to prepare rubusoside | |
| CN104844819A (en) | Modified polyimide film and modified polyimide precursor composite film waste material recovery processing method | |
| KR20100091157A (en) | Preparation of epsilon copper phthalocyanine of small primary particle size and narrow particle size distribution | |
| US2797215A (en) | Production of type a riboflavin crystals | |
| US10556970B2 (en) | Method for preparing high transparent low acyl gellan gum | |
| CN102382072A (en) | Method for refining D-cycloserine | |
| CN102079883B (en) | Novel process for extracting capsanthin and chilli extract by composite solvent | |
| KR102367735B1 (en) | Purifying method of Boron Nitride Nanotube using shear stress | |
| CN102731340A (en) | Preparation method of demethyl aureomycin hydrochloride | |
| CN109097025B (en) | Preparation method of adjustable fluorescent nitrogen dots | |
| CN105017560A (en) | Waste recovery processing method for modified polyimide precursor composition film | |
| TWI466956B (en) | Process of preparing copper phthalocyanine particles exhibiting alpha crystallographic form | |
| KR20170036231A (en) | Purifying method of dodecanedioic acid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20200313 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |